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Preparation method of furoic acid

A technology of furoic acid and furfural, which is applied in the field of chemical substance preparation, can solve problems such as poor raw material utilization, many waste products, and large safety hazards, and achieve the effects of increasing selectivity, mild reaction conditions, and improving yield

Active Publication Date: 2021-02-02
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The oxidant oxidation method mainly uses equivalent oxidizing reagents such as potassium permanganate, sodium hypochlorite, hydrogen peroxide, etc. as the oxidant, which has great safety hazards and many waste products, and is not suitable for industrial production; the Cannizarro disproportionation method generates furfuryl alcohol in equal amounts while producing furfural, and the raw material utilization The efficiency is poor, so it is not suitable for industrial production; the metal oxide catalytic oxidation method is suitable for industrial production, but this method also needs to be carried out under alkaline conditions, so by-products furfuryl alcohol and humin are inevitably generated. Currently, metal oxides are used as There are many reports on the preparation of furoic acid by catalyst, but the reuse rate of catalyst is low

Method used

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  • Preparation method of furoic acid
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  • Preparation method of furoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 1mmol of furfural, 10mL of dimethyl sulfoxide, 10mol% Chimassorb 944 and 10mol% sodium tungstate into a 25ml autoclave. After tightening the screws, fill with oxygen. After three replacements, fill the oxygen pressure to 2MPa and raise the temperature under magnetic stirring. React at 80°C for 12 hours. After the reaction is completed, cool to room temperature, add N,N-dimethylformamide as an internal standard, add methanol to dilute, and detect by gas chromatography. The specific detection conditions are as follows: GC (2104, Shimazu, FID) equipped with DB-FFAP (30m x 0.25μm x 0.32mm) chromatographic column for detection of product content. The vaporization temperature was set at 270°C, the detection temperature was set at 270°C, the oven temperature was set at 120°C, kept for 1 minute, then raised to 230°C within 8 minutes, and kept for 8 minutes. The yield of furoic acid was 84%. The NMR spectrum of the prepared furoic acid is as follows figure 1 shown.

Embodiment 2

[0025] The specific reaction process and detection method are the same as in Example 1, except that sodium tungstate is changed to vanadyl sulfate, and the yield of product furoic acid is 72%.

Embodiment 3

[0027] The specific reaction process and detection method are the same as in Example 1, except that sodium tungstate is changed to vanadium pentoxide, and the yield of product furoic acid is 89%.

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Abstract

The invention discloses a preparation method of furoic acid. The preparation method comprises the following step: subjecting furfural, a light stabilizer, a cocatalyst and a solvent to reacting in thepresence of an oxygen source to obtain furoic acid. The method provided by the invention has the advantages of high selectivity, few byproducts, mild reaction conditions and certain industrial application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical substance preparation, in particular to a preparation method of furoic acid. Background technique [0002] Furfural is an important biomass-derived chemical and can be used as a biomass-based platform compound to prepare a variety of important chemicals. It can be used as a plasticizer, thermosetting resin, etc. in the plastics industry; it can be used as a preservative in the food industry; it can also be used as an intermediate for coating additives, medicines and spices, etc., which are usually produced by oxidation of furfural. [0003] There are generally three processes for preparing furoic acid from furfural oxidation: one is oxidant oxidation, the other is catalytic oxidation, and the other is Cannizarro disproportionation. The oxidant oxidation method mainly uses equivalent oxidizing reagents such as potassium permanganate, sodium hypochlorite, hydrogen peroxide, etc. as the oxidant, wh...

Claims

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Application Information

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IPC IPC(8): C07D307/68
CPCC07D307/68Y02P20/584
Inventor 傅尧李兴龙徐冬冬沈鸿波
Owner UNIV OF SCI & TECH OF CHINA
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